Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → tert-Butyl [3-(2-chloro-5-fluorocarbonylpyrimidin-4-ylamino)propyl]-carbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Cyanuric fluoride | HCID 12664 | — |
| 반응물 | 4-(3-tert-Butoxycarbonylaminopropylamino)-2-chloropyrimidine-5-carboxylic acid | HCID 86673137 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | tert-Butyl [3-(2-chloro-5-fluorocarbonylpyrimidin-4-ylamino)propyl]-carbamate | HCID 86673139 | 98% |
반응 단계
To a suspension of 4.91 g (14.85 mmol) of the product prepared in step 11.1 in 75 mL of dichloromethane are added 2.07 g (14.85 mmol) of triethylamine and then 1.88 mL (22.28 mmol) of cyanuric fluoride. The mixture is stirred at room temperature for 2 hours and the solution is diluted with 100 mL of dichloromethane. The organic phase is washed three times with 100 mL of ice-cold aqueous NaHCO3, dried over MgSO4, filtered and concentrated under vacuum. 4.56 g of the expected product are obtained, and are used directly in the following step. Yield=98%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08975250B2 |
| 출처 데이터셋 | uspto-grants-2015_03 |
| ORD ID | ord-15ab6af9169a447cab03022dd481ae2a |
| 출처 메모 | uspto-grants-2015_03 |